Manufacture



Patented Oct. 29, 1946 1 v i UNl'l'ED STATES PATENT OFFICE MANUFACTURE Saul Kaplan, Rutherford, N. J., assignor to Onyx Oil & Chemical Company, a' corporation of Delaware No Drawing. Application September 12, 1942, Serial No. 458,172

5 Claims. (Cl. 106135) 1 2 This invention relates to improvements in the gum arabic or gelatin or some similar material is art of imparting scroop to fabrics. It includes used as the film-forming protective colloid, it is y new compositions which are useful for that purordinarily desirable to use a preservative. l pose, as well as the process by which scroop is The acid materials to which reference has been imparted to the fabrics and the treated textiles. made ordinarily increase th effectiveness of the Of particular importance is the application of the other constituents in imparting scroop to the texinvention to knitted rayon, although yarn or tile. Some of them have a preservative action other fabrics or textiles may be treated in acand so permit a decrease in the amount of precordance with the invention. servative required. Acid materials are also de- Scroop is a characteristic feel or texture of fab- 0 sirable because they neutralize any alkaline marics perhaps best characterized as the'crisp rustle terials left on the textile in processing prior to the of silk and other fabrics. It is common to treat scrooping treatment. many fabrics, particularly rayon and silk, to im- The mono-esters which substantially consti' part or increase their scroop. For this purpose tute the disperse phase of the new emulsions are silk is treated with soap and then with acid to libesters of certain higher fatty acids, that is, those crate fatty acids on the fibers. Weak organic containing 10 to 14 carbon atoms, such as lauric acids, such as formic, acetic, lactic, or tartaric acid, or mixtures containing such acids in preacids are sometimes used alone, particularly with dominating quantities, such as the mixed fatty silk, as these products are not ordinarily sufllacids of coconut oil, palm kernel oil, babassu oil, ciently effective with rayon. Emulsions of the and the 10 to licarbon atom cut of the acidic higher fatty alcohols, such as oleyl alcohol, are productresultlng on the oxidation of petroleum, used for imparting scroop to fabrics, particularly with ethylene or propylene glycol. rayon. 4 Advantageously the disperse phase consists only In accordance with the present invention, of such a fatty acid ester, or mixture thereof, toemulsions of certain esters of higher fatty acids gether with a small amount of an emulsifying are used to impart scroop to textiles, and particuagent if an oil-soluble emulsifying agent is used. larly knitted rayon. These emulsions are. of the However, the ester may be extended by: means of oil-in-water type, with the disperse phase coma mineral oil, such as one of a viscosity of 50 to prising a mono-ester of a higher fatty acid hav- 100 seconds Saybolt, at 100 F. Such a mineral ing 10 to 14 carbon atoms,- or a mixture containoil may be used in quantities up to 50 or 60% ing the same, with ethylene or propylene glycol, without reducing the scrooping eflect too radicalthe continuous phase being an aqueous medium ly. Relatively small quantities of waxes may containing a film-forming protective colloid such also -be included in the disperse phase, but if as a gum, gelatin. or the like. waxes are used in quantities over about 10%, the

In addition to thes necessary constituents, scroop is decreased and emulsification difilculthe emulsions may contain other material such as ties may be encountered with some protective colemulsifying agents, preservatives, and weakly loids.

, acidic material, such as a weak organic acid or The continuous phase consists of an aqueous an acid salt of an organic acid or an acid salt of solution of a film-forming protective colloid.

an inorganic acid, such as aluminum sulfate. 40 Among the colloids which maybe used are gela- .The use of emulsifying agents is ordinarily detin (a gelatin or glue), gum arable, gum ghatti,

,, sirable to reduce the time and power required to casein, methyl cellulose, gum tragacanth, gum produce a stable emulsion; but care must be karaya, gum shiraz, starch, soluble alginates, taken that the emulsifying agent used is compatpolyvinyl alcohol, locust bean gum, casein-alumiible with the other constituents of the emulsions num formate complex, and the like. and other materials in conjunction with which Among the acidic materials which may be inthe emulsions may be used. Many emulsifying cluded in the continuous phase, if the acidic maagents exert a decided softening effect which terial is used, are the weak organic acids, such as radically reduces the scrooping effect if used in formic, acetic, lactic, glycolic, citric, tartaric,

any substantial quantity; but ordinarily effective ph i m l l succinic. and malic acid; acidic emulsions can be obtained with the use of quansalts of organic acids, such as aluminum formate titles of emulsifying agent too small to have this or acetate, (both normal and basic salts), ammodeleterious result. nium lactate, ammonium oxalate, zinc acetate Preservatives in some instances are required and Zinc formate; and acidic salts of inorganic because of the protective colloids used, Thus if acids, such as aluminum sulfate, zinc sulfate, am-

. pared from the following:

monium sulfamate, aluminum sulfamate, zinc sulfamate, monammonium phosphate, and dl-' ammonium phosphate.

Both oil-soluble and water-soluble emulsifying agents may be used, including the petroleum sulfonates, mahogany soaps, fatty alcohol sulfates, salts of alkylated naphthalene sulfonates, sulfocarboxylic esters (such as dioctyl sodium sulfosuccinate) -acylated protein degradation products, higher alcohol-secondary sulfates, alkyl' Example 1.-A scrooping composition is prepared from the following:

Pounds Ethylene glycol mono-laurate 20;0 Gela n 2.0" Sodium diisopropyl naphthalene sulfonate 0.1 Sodium pentachlorphenate 0.2 Water 7.7.7

The gelatin is soaked in part ofthe water, and the mixture is heated to dissolve it. The sodium diisopropyl naphthalene sulfonate is dissolved in 2 parts of the water, and added to the gelatin. The ethylene glycol mono-laurate, at a temperature of from 30 to 35 C., is then added to this mixture while it is agitated rapidly, such as with a turbo mixer. The balance of the water and preservative is then added; The mixture may then, if desired, be passed through a colloid mill if creaming occurs on prolonged storage, agitation will restore its homogeneity, and its usefulness is unimpaired.

Example 2.-A scrooping composition is prepared from the following:

Pounds Propylene glycol mono-laurate 15.0 Gelatin- 8.0 Sodium diisopropyl naphthalene sulfonate 0.1 Sodium orthophenyl phenate 0.2 Water 67.? Aluminum formate', 15 B 9.0

The above materials are mixed as in Example 1, the aluminum formate being added last, the emulsion being heated to about 40? C. before its addition.

Example 3.The sodium diisopropyl naphthalene sulfonate in Example 1 is replaced by 1 to 3 lb. of potassium oleate or triethanolamine oleate, or by M1110 1 lb. of mahogany soap. The last two may be dissolved in the ethylene glycol monolaurate, if desired.

Example 4-.A scrooping composition is pre- Pounds Propylene glycol mono coconut fatty acid ester Gum arabic solution 50% suitably preserved-.. 6

I Water '79 The materials are mixed and suitably emulester 16 Casein-aluminum formate complex 50 Water 34 The ethylene glycol mono coconut fatty acid ester is emulsified in the casein-aluminum formate complex at the temperature of liquefaction of the complex, and then the water is added.

Example 6.A skein of cuprammonium yam, previously freed from oil and size by a conventional boil-ofi, and which may have subsequently been dyed, is worked in a bath containing 1 to 5% of any of the compositions of the previous examples. The percentage is based on the weight of the skein, and the amount of the water used may be from 10 to 25 times the weight of the skein. After 15 minutes, the skein is extracted, and dried, It possesses a firm crunchy feel. The effect is somewhat enhanced if from 0.5% to 2% of formic acid is added to the bath a. few minutes :Examples 1 to 5 in a suitable apparatus, such as a .rnangle. Upon drying, the goods have a'goodscroop, and in the case of some constructions, which are brushed to produce 'a nap, still retain the scroop, despite the mechanical working.

Example 8.-Rayon knit oods are dyed, afterscouring, in a reel type machine, and the dye bath is dropped. The machine is filled with water at about 100 F., and 2% of an emulsion of any of Examples 1 to 5 (based on the weight of the goods) is added; After running15 minutes, the liquor is dropped, the goods extracted, and

dried. The effect may be increased by adding,-

.or homogenizer. A stable emulsion results, and

with the emulsion, about@. 0 .5% of maleic acid, based on the weight of the goods.

Naturally some of the emulsions illustrated above are more eihcient than others, and some tend to produce a more. lastingxscroop than others. In general, an increase in thequantity of ester in an emulsion increases its effectiveness, those containing amounts of ester ranging up to 40% generally giving a better and more lasting scroop than those containing 10% or less, if used at the same concentration.

In formulating any emulsion to be used in impartingscroop to a fabric, care must be taken that the various constituents are compatible and also that they are compatible with other materials in conjunction with which they are to beused. Thus, if the film-forming protective colloid used is gum arabic, aluminum acetate should not .be included in the emulsion as its use will lead to precipitation when the emulsion is diluted, if not before. Similarly, where the emulsions are to be used in conjunction with other finishes, such as water repellents, fire proofing compounds, and weighting compositions, ingredients which are incompatible with these other finishes should not be included in the emulsions.

When an emulsifying agent is used in preparing the emulsion, it is usually best to make 8- perse phase. a mono-ester of a glycol having from 2 to 3 carbon atoms with a higher fatty acid having to 14 carbonatoms, and a continuous phase comprising an aqueous solution of a filmforming protective colloid, and a water-soluble organic carboxylic compound selected from the group consisting of carboxylic acids and their acidic reacting salts.

'2. An oil-in-water emulsion having, as the disperse phase, a mono-ester of a glycol having from 2 to 3 carbon atoms'with a higher fatty acid hav ing 10 to 14 carbon atoms, and a continuous phase comprising an aqueous solution of a filmforming protective colloid, and a water-soluble acid reacting inorganic salt selected from the ing 10 to 14 carbon atoms, and a continuous phase comprising an aqueous solution of a filmiorming protective colloid, and a water-soluble organic carboxylic compound selected from the group consisting of carboxylic acids and their acidic reacting salts, and an organic emulsifying agent.

4. An oil-in-water emulsion having, as the disperse phase, a mono-ester of a glycol having from 2 to 3 carbon atoms with a higher fatty acid having 10 to 14 carbon atoms, and a continuous phase comprising an aqueous solution of a filmforming protective colloid, and a Water-soluble acid reacting inorganic salt selected from the group consisting of soluble sulfamates, sulfates and phosphates, and an organic emulsifying agent.

- 5. A new composition of matter comprising a water-in-oil emulsion with a disperse phase comprising propylene glycol monolaurate and a continuous phase comprising an aqueous solution of a water-soluble protein selected from the class consisting of gelatine and glue, and sodium diisopropyl naphthalene sulfonate.

SAUL KAPLAN. 

